hi 84500 free & total sulfur dioxide …...4 5 significance of use ph 3.0 3.1 3.2 3.3 3.4 3.5...

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1 Instruction Manual HI 84500 FREE & TOTAL SULFUR DIOXIDE MINITITRATOR for wine analysis www.hannainst.com

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Page 1: HI 84500 FREE & TOTAL SULFUR DIOXIDE …...4 5 SIGNIFICANCE OF USE pH 3.0 3.1 3.2 3.3 3.4 3.5 3.6 3.7 3.8 3.9 Free SO 2 14 18 22 28 35 44 55 69 87 109 A dedicated HELP key aids in

1

Instruction Manual

HI 84500FREE & TOTAL SULFUR DIOXIDE

MINITITRATORfor wine analysis

www.hannainst .com

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All rights are reserved. Reproduction in whole or in part is prohibited without the written consentof the copyright owner, Hanna Instruments Inc., Woonsocket, Rhode Island, 02895, USA.

TABLE OF CONTENTS

PRELIMINARY EXAMINATION................................................................................................. 4

GENERAL DESCRIPTION ........................................................................................................ 4

SPECIFICATIONS ................................................................................................................... 6

PRINCIPLE OF OPERATION .................................................................................................... 7

FUNCTIONAL DESCRIPTION ................................................................................................... 8

TITRATOR STARTUP ........................................................................................................... 10

SETUP MENU .................................................................................................................... 11

GUIDE TO DISPLAY CODES ................................................................................................... 15

ELECTRODE PREPARATION .................................................................................................. 18

DOSING PUMP INSTALLATION ............................................................................................. 19

DOSING PUMP PRIME PROCEDURE ..................................................................................... 19

ELECTRODE CHECK PROCEDURE .......................................................................................... 21

PUMP CALIBRATION PROCEDURE ........................................................................................ 21

FREE SO2 MEASUREMENT PROCEDURE ................................................................................ 24

TOTAL SO2 MEASUREMENT PROCEDURE .............................................................................. 27

ORP MEASUREMENT .......................................................................................................... 32

PC INTERFACE AND DATA TRANSFER ................................................................................... 34

TROUBLESHOOTING GUIDE ................................................................................................ 35

ELECTRODE CONDITIONING AND MAINTENANCE .................................................................. 36

ACCESSORIES ..................................................................................................................... 38

WARRANTY ........................................................................................................................ 39

Dear Customer,

Thank you for choosing a Hanna Instruments product.

Please read this instruction manual carefully before using this instrument. This manual willprovide you with the necessary information for correct use of this instrument, as well as a preciseidea of its versatility.

If you need additional technical information, do not hesitate to e-mail us at [email protected] view our worldwide contact list at www.hannainst.com.

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SIGNIFICANCE OF USE

Hp 0.3 1.3 2.3 3.3 4.3 5.3 6.3 7.3 8.3 9.3

OSeerF2

41 81 22 82 53 44 55 96 78 901

A dedicated HELP key aids in setup, calibration, status and troubleshooting.Other features:

• ORP meter• Stirrer speed control• Graphic mode to display the titration data• Data can be stored using the log feature and then exported to a USB stick or transferred

to a PC using the USB connection• Log on demand for up to 400 samples (200 for mV measurements; 200 for titration

results)• GLP feature, to view calibration data for the pump

Wine makers add sulfur dioxide to wine in order to inhibit bacteria and wild yeast growth and toserve as an antioxidant to prevent browning.When SO

2 is added to wine, a portion of it becomes immediately bound while a remaining portion

is unbound SO2. The portion that is unbound is also called free; it is responsible for protecting the

wine. The bound and unbound SO2 together are referred to as total SO

2.

The relationship between the amount of SO2 added and the amount of free SO

2 is complex. This

relationship is governed by the total amount of SO2 in the wine. The exact relationship between free

and bound will vary wine to wine. The amount of free SO2 depends on how much is added, how much

was present before the addition and how much was immediately bound.Free SO

2 exists in two forms. Bisulfite (HSO

3¯) is the predominante form but is relatively ineffective.

Molecular SO2 is the minor form and is responsible for protecting the wine.

The amount of molecular SO2 available in wine is depended on the amount of free SO

2 present and

the pH. Typically 0.8 ppm of molecular SO2 provides adequate protection against bacteria growth

and oxidation. In order to obtain this value for a wine sample that has a pH of 3.2 you would need22 ppm of free SO

2, if the pH was at 3.5 you would need double, 44 ppm.

Molecular SO2 can be detected by human senses at about 2.0 ppm. This level is needed for

maximum protection of wine. Higher levels are needed for sweet and most notable, botrytised wine.The HI 84500 can be used to test for free and total SO

2 in all wines, including red, which are

difficult to test using traditional methods associated with a distinctive color change to determine the

end point.

Please examine this product carefully. Make sure that the instrument is not damaged. If anydamage occurred during shipment, please notify your Dealer.

Each HI 84500 minititrator is supplied complete with:

• HI 84500-70 Reagent Kit for SO2 determination

• HI 3148B ORP electrode

• HI 7082 Electrode Fill Solution (30 mL)

• Two 100 mL beakers

• Two 20 mL beakers

• Scissors

• Dosing Pump Valve

• 5 mL Syringe

• 1 mL Plastic Pipette

• Tube set (aspiration tube with titrant bottle cap and dispensing tube with tip)

• Stir bar

• Power Adapter

• Two sachets of cleaning solution for wine deposits

• Two sachets of cleaning solution for wine stains

• Instruction manual

Note: Save all packing material until you are sure that the instrument works correctly.Any defective item must be returned in its original packing.

PRELIMINARY EXAMINATION

The HI 84500 is a low-cost, easy to use, microprocessor-based automatic titrator that benefitsfrom Hanna’s years of experience as a manufacturer of analytical instrumentation.

The instrument incorporates a simple and reliable dosing pump which ensures high dosingreproducibility. Pump calibrations, performed with the provided Hanna reagents, assure theaccuracy of the instrument.

The instrument comes with a preprogrammed method for Free and Total Sulfur Dioxidemeasurements in wine. The instrument uses a powerful algorithm which analyzes the shape ofthe electrode response in order to determine when the titration has reached completion.

The HI 84500 provides a simple user interface. By simply pressing the Start key in Titrationmode, the instrument will automatically titrate the sample to the equivalence point and theresults are immediately displayed in ppm. Another titration can be started immediately bypressing Restart.

GENERAL DESCRIPTION

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PRINCIPLE OF OPERATION

The HI 84500 determines the free and total sulfur dioxide concentration in wine using the Rippermethod. Excess iodide added to the wine sample reacts with iodate introduced by the titrant toproduce iodine.

IO3

- + 5I- + 6H+

→ 3I2 + 3H

2O

The iodine produced in the sample then reacts with sulfur dioxide in the wine according to the redoxreaction below:

H2SO

3 + I

2 → H

2SO

4 + 2HI

The HI 84500 utilizes an ORP electrode to monitor the redox titration. The integrated algorithmdetects when the reaction is complete (equivalence point). The volume of titrant required to reach theequivalence point, the titrant concentration and the sample size are used to calculate the sulfurdioxide concentration in the wine sample.

Titrator Range Low Range: 1.0 to 40.0 ppm of SO2

High Range: 30 to 400 ppm of SO2

Resolution Low Range: 0.1 ppm

High Range: 1 ppm

Accuracy Low Range: 3% of reading or ±0.5 ppm @ 25 °C, whichever is greater

High Range: 3% of reading or ±1 ppm @ 25 °C, whichever is greater

Sample volume 50 mL

Titration method Ripper method

Principle Equivalence point redox titration

Pump speed 10 mL/min

Stirring speed 700 rpm

Log data Up to 200 samples

ORP meter ORP meter -2000.0 to 2000.0 mV

ORP Resolution 0.1 mV

ORP Accuracy ± 1 mV

Log data Up to 200 samples

ORP Electrode HI 3148B

Environment 0 to 50 °C (32 to 122 °F); max 95% RH non-condensing

Power supply 12 Vdc power adapter

Dimensions 235 x 200 x 150 mm (9.2 x 7.9 x 5.9”)

Weight 1.9 kg (67.0 oz.)

REQUIRED REAGENTS

Code Description

HI 84500-50 Low Range Titrant

HI 84500-51 High Range Titrant

HI 84500-55 Calibration Standard

HI 84500-60 Acid Reagent

HI 84500-61 Alkaline Reagent (Total SO2)

HI 84500-62 Stabilizer Packet

SPECIFICATIONS

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ESC - used to leave the current screen and to return either to the previous screen or to themain screen. In Setup menu, exits a parameter without changing the value.

/ - used to modify the parameter values, to scroll the information displayed whileviewing a help screen or to move between the options from the instrument’s Setup menu

CAL - used to access the Pump calibration

HELP - used to access/exit the instrument’s contextual help

LOG - used to save the current mV-ORP reading in ORP meter mode and the titration result

MENU - used to enter Setup, Recall or GLP selection menu, while instrument is in ORP orTitration mode

STIR - used to start/stop the stirrer

Note: The stirrer starts automatically during pump calibration and titration, it cannotbe stopped by pressing STIR key.

GUIDE TO INDICATORSDuring the instrument’s operation information is displayed on the LCD.

Displayed icons:

Unstable reading.Stirrer on. Pump running.

Parameter can be modified.

KEYPAD FUNCTION

1) Current time and instrument mode information (ORP meter or Titrator)

2) Instrument status

3) Virtual option keys4) Stirrer and reading status

5) Main reading information

Stirrer is not working properly.

FRONT VIEW

REAR VIEW

6) ORP Electrode

7) Beaker

8) Dosing pump

9) Power switch

10) Power adapter

11) USB connector (PC interface)

12) USB connector (Storage interface)

13) BNC electrode connector

14) Titrant bottle

15) Syringe

16) Aspiration tube

17) Dosing Pump Valve

FUNCTIONAL DESCRIPTION

OVERHEAD VIEW

1) Titrant bottle

2) Liquid Crystal Display (LCD)

3) Keypad

4) Electrode holder

5) Dispensing tube

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SETUP MENU

The titrator’s setup menu may be accessed from the main screen (meter or titrator mode) bypressing the MENU key, then Setup.

A list of setup parameters will be displayed with currently configured setting.

While in the setup menu it is possible to modify the instrument’s operation parameters. TheARROW keys permit the user to scroll the setup parameters.

Press HELP to view the contextual help.

Press ESC to return to the main screen.

Range Setup

Use Low measurement range for 1.0 - 40.0 ppm.

Use High measurement range for 30 - 400 ppm.

Use the appropriate titrant for each range.

To ensure a high accuracy, it is recommended torecalibrate the pump after the valve, titrant orelectrode has been changed.

Derivative Filter

Select Enable to activate or Disable to deactivatethe derivative filter function.

If enabled, a filtering procedure of first derivate isapplied that reduces the influence of mV noise thatcan appear due to chemical system properties, suchas slow reaction or unbuffered wine sample,electrode response.

Threshold HR

Press Modify to change the value.The threshold value must be set by user in acordingwith wine sample analysis. It represents the absolutevalue of the first derivative expressed in mV/mL belowwhich the detection algorithm does not search toequivalance point. Range between 10 and 10000mV/mL. The recommended value for the threshold isaround 40% of the estimated maximum absolutevalue of the first derivate.Use the ARROW keys or / to increase/decrease the value. Press Accept to confirm the valueor ESC to return to the setup menu.

TITRATOR STARTUP

This is a general outline of the steps required to perform a titration. The following topics areexpanded upon in each section that follows.

• Place the instrument on a flat table. Do not place the instrument in direct sun light.

• Connect the power adapter to the instrument.

• Turn the instrument ON using the power switch from the rear panel of the instrument.

• Set up the instrument. See the “Setup Menu” section for details.

• Connect the ORP sensor to the instrument.

• Connect the tubes and the valve. See the “Dosing Pump Installation” section for theprocedure.

• Remove the titrant bottle cap and replace it with the bottle cap with tubes. Place the titrantbottle in the appropriate place on the titrator top.

Note: Different titrants are required based on the concentration. See “Pump Calibration Procedure”for details.

• Prime the syringe. To assure high accuracy, verify there are no air bubbles in the syringe ortubing.

• Calibrate the pump.

Note: Different volumes of standard are required based on the concentration. See “PumpCalibration Procedure” for details.

• Prepare the sample.

• Run a titration and log sample results.

DOSING PUMP

The dosing pump is based on a valve that automatically moves the titrant between the titrantbottle and syringe when filling the syringe and between the syringe and sample whendispensing. A replaceable 5 mL plastic syringe is used to limit the amount of titrant used per testto ensure the highest possible accuracy. Before a set of titrations, it is necessary to prime thedosing system.

Note: Once titrations have been completed, the dosing system should be cleaned with deionizedwater using the prime feature.

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Key Beep

Select Enable to activate or Disable to deactivatethe Key Beep function.

If enabled, a short beep will be heard every time akey is pressed.

Error Beep

Select Enable to activate or Disable to deactivatethe Error Beep function.

If enabled, a beep will be heard when an errorcondition occurs.

Decimal Separator

This option allows the user to select the symbolused for a decimal separator.

LCD Contrast

This option is used to set the display’s contrast.Press Modify to change the display’s contrast.The default value is 8.

Use the ARROW keys or / to increase/decrease the value. Press Accept to confirm the valueor ESC to return to the setup menu.

Time

Press the Modify key to change the time and timeformat.

Press Format to switch between 12 hour (am/pm)and 24 hour mode.Press to highlight the value to be modified. Usethe ARROW keys to change the value. Press Acceptto confirm the new value or ESC to return to thesetup.

Date

Press the Modify key to change the date and dateformat.

Threshold LR

Press Format to cycle between the available dateformats.Press to highlight the value to be modified. Usethe ARROW keys to change the value. Press Acceptto confirm the new value or ESC to return to thesetup.

LCD BacklightPress Modify to change the backlight level.

The default value is 3.

Press Modify to change the value.Note: To find the optimal threshold value follow the

next steps:• Set the maximum threshold value for selected range.• Run the titration to reach the maximum titration volume.• Use the dmV/dmL value displayed on the screen

to estimate the optimal threshold (recommendedvalue is 40% of this value).

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Restore Factory Settings

Press Select to restore the factory settings.

Press Yes to confirm the restore process or No toreturn without restoring.

Press ESC to return to the setup menu.

GUIDE TO DISPLAY CODES

Titration screen when a titration is in progress.

Titration screen display.

This screen appears when the instrument is turnedon during the initialization process.

Prime burette screen.

Press the corresponding virtual option key to changethe language.

If the selected language cannot be loaded, thepreviously selected language will be reloaded.

If no language can be loaded at startup the instrumentwill work in “safe mode”. In “safe mode” allmessages are displayed in English. Tutorial and helpinformation are not available.

Language

Press Select to view the firmware version, languageversion, mV factory calibration date and time,method version.

Meter Information

Tutorial

Enable or Disable the Tutorial. This helpful tooloffers additional information during calibration andtitration.

Press ESC to return to the setup menu.

Use the ARROW keys or / to increase/decrease the backlight level.

Press Accept to confirm or ESC to return to thesetup menu.

Prime burette screen when the dosing system isrunning.

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The calibration was outside the acceptable limits.Prepare a new standard and try again.

This error message appears when the input reading(mV) exceeds the input limits (± 2000.0 mV).

This screen is displayed when the instrument is intitration mode. Press Start to begin a titration, Meterto enter ORP meter mode or Prime to enter into theprime function.

TITRATION MESSAGES

The titration result, expressed as the concentration ofsulfur dioxide in ppm (mg/L), is displayedautomatically at the end of the titration. Press Restartto start another titration or ESC to return to the mainscreen.

This screen appears when the stirrer is not workingproperly. Check the stir bar and beaker content.Press Restart to try again.

This error message appears when the pump is notworking properly. Check the tubing, valve andsyringe. Press Restart to try again.

PUMP CALIBRATION MESSAGES

Pump calibration is initiated by pressing the Startkey.

This error message appears when the pump is notworking properly. Check the tubing, valve andsyringe. Press Restart to try again.

This error message appears during pump calibrationwhen the end point can not be reached and themaximum amount of titrant is exceeded. Checkstandard, electrode and/or dosing system and tryagain.

This screen appears while pump calibration is inprogress. Press ESC or Stop key to return to thePump Calibration screen.

This screen appears when pump calibration iscomplete.

This error message appears when the input reading(± 2000 mV) exceeds the input limits during atitration.

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DOSING PUMP INSTALLATION

To install the dosing pump follow the procedure below:

• Extend the plunger on the 5 mL syringe to its maximum volume.

• Place the syringe in the dedicated spot on the top of the meter (1).

• Arrange the bottom of the syringe into the holder on the pump (2). Once the syringe is in placelower the barrel until it sits flush on the holder.

• Put the o-ring and syringe-fixing nut over the syringe (3) and turn clockwise to secure it in place (4).

• Place the valve on the top of the syringe (5). Ensure it fits securely.

• Insert the aspiration tube into the left side of the valve (6) and replace the titrant bottle cap withthe attached cap (7).

• Insert the dispensing tube into the top of the valve (8).

DOSING PUMP PRIME PROCEDURE

Prime cycle should be performed:

• if you notice there is no titrant in the tip

• whenever the dosing system tubes are replaced

• whenever a new bottle of titrant is used

• before starting a pump calibration

• before starting a series of titrations

The prime cycle is used to fill the syringe before starting a set of titrations.

Two rinse cycles of the syringe are shown in the figure below. The dispensing tube is connected tothe top of the valve and the aspiration tube on the left side.

ELECTRODE PREPARATION

PREPARATION PROCEDURE

Remove the electrode protective cap.

DO NOT BE ALARMED IF ANY SALT DEPOSITS ARE PRESENT. This is normal with electrodes andthey will disappear when rinsed with distilled/deionized water.

During transport tiny bubbles of air may have formed inside the glass bulb. The electrode cannotfunction properly under these conditions. These bubbles can be removed by "shaking down" theelectrode as you would do with a glass thermometer.

If the bulb is dry, soak the electrode in HI 70300 Storage Solution for at least one hour.

This screen appears when the stirrer is not workingproperly. Check the stir bar and beaker content.Press Restart to try again.

This error message appears when the pump is notworking properly. Check the tubing, valve andsyringe. Press Restart to try again.

This screen appears when the first derivative isunder the threshold value. Check the sample andthreshold settings.

This screen appears when the sample concentrationis out of range.

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Pump calibration must be performed every time the syringe, pump tube, the titrant bottle or the ORPelectrode is changed. A pump calibration is recommended before each set of titrations or after thetitrator is left idle for several hours.

• Press MENU, select Setup and select the corresponding range according to the table below:

• Ensure the pump is primed with the correct titrant for the selected range (HI 84500-50 LowRange Titrant or HI 84500-51 High Range Titrant).

Sample preparation: Use a clean pipette to precisely add the appropriate amount ofHI 84500-55 Calibration Standard to a clean beaker as indicated below:

PUMP CALIBRATION PROCEDURE

egnaRwoL egnaRhgiH

mpp0.04ot0.1 mpp004ot03

Low Range (Free & Total SO2) - 1 mL

High Range (Free & Total SO2) - 10 mL

Note: Failure to use a clean pipette will result in erroneous readings.

• Fill the beaker up to the 50 mL mark with the distilled ordeionized water.

• Fill the 20 mL beaker up to the 5 mL mark with the HI 84500-60Acid Reagent and add the contents to the 100 mL beaker.

• Add the contents of one packet of HI 84500-62 StabilizerPacket to the sample beaker.

ELECTRODE CHECK PROCEDURE

Before taking any measurements with the HI 84500 minititrator, it is recommended to checkthe HI 3148B ORP electrode using the following steps:

• Press Meter to enter mV mode.

• Pour roughly 15 mL of HI 7021 into a 20 mL beaker. This does not need to be exact, aslong as the PTFE junction is covered by the solution.

• Place the electrode in the solution, stir gently for a few seconds and verify the mV reading.If the mV reading is 240 ± 20 mV this indicates the electrode is in good condition and canbe used for titrations. A mV reading of 240 ± 30 mV indicates the electrode is beginningto drift. Follow the “Electrode Conditioning and Maintenance”, Probe Maintenance sectionon page 32. If the mV reading is greater than 240 ± 40 mV replace the electrode.

• Remove the electrode from the solution and rinse thoroughly with deionized or distilled water.

Note: • The aspiration tube must be inserted in the titrant bottle. The dosing tip must be placedover a rinse beaker.

• Before starting the prime procedure, make sure you are using the appropriate titrantsolution for the selected range.

• To prime the burette, select Prime option from Titration mode.• Adjust the rinses number by pressing the and keys and press Start.

• The number of syringe rinses can be set between 1 and 5 (at least three rinses are recommendedto ensure that the air bubbles are completely removed).

• To pause the prime process press the Pause key; to continue press the Continue key. To stop theprime process press the Stop key.

Note: This error message appears when the pump isnot working properly. Check the tubing, valveand syringe. Press Restart to try again.

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• Press Start, wait for the syringe to refill.

• Place the stir bar in the beaker and put the beaker in theminititrator top.

• Place the probe holder on the top of the beaker and secure itby turning clockwise.

• Rinse the ORP electrode with deionized water and immerseinto the sample until the PTFE reference junction is completelysubmerged. Be sure that the tip of the electrode is nothitting the stir bar. If necessary additional distilled ordeionized water can be added.

• Insert the dosing tip into the titrant tube sleeve. IT ISCRITICAL THAT THE TIP BE IMMERSED APPROXIMATELY0.25 CM (0.1”) INTO THE SOLUTION BEING TITRATED.

• Press Continue to begin the calibration and Stop to abort it.

• At the end of the calibration, “Calibration Completed“appears on display. To repeat the calibration press Restartand ESC to return to the main screen.

Note:

• If an erroneous situation is encountered duringthe calibration, an error message is displayedand the calibration can be restarted by pressingRestart. Prepare a new standard, rinse electrodeand dosing tip and try again.

• If the calibration doesn’t complete and themax titrant volume of titrant is reached, anerror message will be displayed. Thecalibration can be restarted by pressing Restart.Prepare a new standard, rinse the electrodeand dosing tip and try again.

• This error message appears when the inputreading (mV) exceeds the input limits(± 2000.0 mV).

• This screen appears when the stirrer is notworking properly. Check the stir bar and beakercontent. Press Restart to try again.

• This error message appears when the pump isnot working properly. Check the tubing, valveand syringe. Press Restart to try again.

• Press CAL key.

Note: DO NOT PLACE THE TIP INTO THE CALIBRATION BEAKER, PLACE THE TIP OVERA WASTE BEAKER. A SMALL AMOUNT OF TITRANT IS DISPENSED WHEN THEPUMP RESETS.

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• The instrument will continuously update the concentration on the display. The value will bedisplayed blinking. When the reading is under range “----” symbol appears blinking.

• The titration curve can be visualized during a titration by pressing Plot ON. Press Plot OFF toexit this mode.

• At the end of the titration the instrument displays the concentration in ppm of SO2. The titration

curve can be viewed by pressing Plot ON. Press Plot OFF to exit this mode.

• Place the probe holder on the top of the beaker and secure it byturning clockwise.

• Rinse the ORP electrode with deionized water and immerse intothe sample until the PTFE reference junction is completelysubmerged. Be sure that the tip of the electrode is not hitting thestir bar.

• Insert the dosing tip into the titrant tube sleeve. IT IS CRITICALTHAT THE TIP BE IMMERSED APPROXIMATELY 0.25 CM (0.1”)INTO THE SOLUTION BEING TITRATED.

• Press Continue to begin the titration and Stop to abort it.

FREE SO2 MEASUREMENT PROCEDURE

• Refer to “Setup Menu” (see page 10) to set up the instrument for your measurement.

• For best accuracy, before taking any measurement, ensure that the pump is calibrated on theselected range following the “Pump Calibration Procedure” (see page 19).

• Select the corresponding range according to the table below:

• Ensure the pump is primed with the correct titrant for the selected range (HI 84500-50 LowRange Titrant or HI 84500-51 High Range Titrant).

Sample preparation: Use a clean pipette to precisely add the appropriate amount of winesample to a clean 100 mL beaker as indicated below:

egnaRwoL)elpmasLm05(

egnaRhgiH)elpmasLm05(

mpp0.04ot0.1 mpp004ot03

Low Range (Free & Total SO2) - 50 mL

High Range (Free & Total SO2) - 50 mL

Note: •The volume of wine added is critical to the measurementaccuracy. Pipettes are recommended.

•Failure to use a clean pipette will result in erroneousreadings.

• Fill the 20 mL beaker up to the 5 mL mark with the HI 84500-60Acid Reagent and add the contents to the 100 mL beaker.

• Add the contents of one packet of HI 84500-62 StabilizerPacket to the 100 mL beaker.

• Press Titrator.

Note: DO NOT PLACE THE TIP INTO THE SAMPLE BEAKER. PLACE THE TIP OVER AWASTE BEAKER. A SMALL AMOUNT OF TITRANT IS DISPENSED WHEN THE PUMPRESETS.

• Press Start to begin a titration.

• Wait for the syringe to refill.

• Place the stir bar in the beaker and put the beaker into the beaker holder.

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• For best accuracy, before taking any measurement, ensure that the pump is calibrated on theselected range following the “Pump Calibration Procedure” (see page 19).

• Select the corresponding range according to the table below:

TOTAL SO2 MEASUREMENT PROCEDURE

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Low Range (Free & Total SO2) - 50 mL

High Range (Free & Total SO2) - 50 mL

Note: •The volume of wine added is critical to the measurementaccuracy. Pipettes are recommended.

•Failure to use a clean pipette will result in erroneous readings.

• Fill the 20 mL beaker up to the 5 mL mark with the HI 84500-61Alkaline Reagent, add the contents to the 100 mL beaker containingthe sample.

• Cover the beaker, swirl and wait for 10 minutes.

• Fill the 20 mL beaker up to the 5 mL mark with the HI 84500-60Acid Reagent, add the contents to the 100 mL beaker containingthe sample.

• Add the contents of one packet of HI 84500-62 Stabilizer Packetto the 100 mL beaker.

• Place the beaker into the beaker holder.

• Press Titrator.

Note: DO NOT PLACE THE TIP INTO THESAMPLE BEAKER. PLACE THE TIP OVERA WASTE BEAKER. A SMALL AMOUNTOF TITRANT IS DISPENSED WHEN THEPUMP RESETS.

• Press Start to begin a titration.

• Ensure the pump is primed with the correct titrant for the selected range (HI 84500-50 LowRange Titrant or HI 84500-51 High Range Titrant).

Sample preparation: Use a clean pipette to precisely add the appropriate amount of winesample to a clean 100 mL beaker as indicated below:

• This error message appears when the pump is not working properly. Check the tubing, valveand syringe. Press Restart to try again.

• Press LOG to record the concentration value and the titration curve into the instrument’smemory. A message will be displayed for a few seconds indicating the amount of free logspace. Up to 200 log samples can be recorded in the instrument’s memory.

• Press Restart to begin a new titration or ESC to return to the titration menu.

• If the concentration exceeds the range limits (>40.0 ppm for Low Range, >400 ppm forHigh Range), the exceeded range limit will be displayed blinking. Another titration can bestarted by pressing Restart.

• “Wrong input” error message appears when the input reading (mV) exceeds the specifiedlimits. The mV value and the concentration will blink indicating an error.

• This screen appears when the stirrer is not working properly. Check the stir bar and beakercontent. Press Restart to try again.

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VIEW/DELETE TITRATOR RECORDED DATA

Press MENU then Recall to access the Titrator logs.

When an external USB storage device is connected, the Export key is displayed. It saves the meterand titrator logs in two text format files on the storage device.

Press Meter or Titrator to view the respective logs.

The instrument will display a list of all the records stored in the log.

Use the ARROW keys to scroll the stored records list.

If the saved concentration was out of range, the “<” or “>” symbols are displayed in front ofthe reading.

TIPS FOR AN ACCURATE MEASUREMENT

The instructions listed below should be followed carefully to ensure measurements are conductedwith the highest possible accuracy and precision.

• IT IS CRITICAL THAT THE TIP BE IMMERSED IN THE SOLUTION BEING TITRATED(APPROXIMATELY 0.25 CM).

• Use a clean, volumetric pipette to measure and transfer the wine sample into the titrationbeaker.

• Calibrate the pump prior to each series of titrations.

• Calibrate the pump if the meter is left idle for several hours.

• Analyze the wine sample immediately after it is obtained.

• Clean the electrode with HI 700635 or HI 700636 cleaning solutions specially designed forthe wine industry.

• Press LOG to record the concentration value and the titration curve into the instrument’smemory. A message will be displayed for a few seconds indicating the amount of free logspace. Up to 200 log samples can be recorded in the instrument’s memory.

• Press Restart to begin a new titration or ESC to return to the titration menu.

• Wait for the syringe to refill.

• Place the stir bar in the beaker and put the beaker into thebeaker holder.

• Place the probe holder on the top of the beaker and secure it byturning clockwise.

• Rinse the ORP electrode with deionized water and immerse intothe sample until the PTFE reference junction is completelysubmerged. Be sure that the tip of the electrode is not hittingthe stir bar.

• Insert the dosing tip into the titrant tube sleeve. IT IS CRITICALTHAT THE TIP BE IMMERSED APPROXIMATELY 0.25 CM (0.1”)INTO THE SOLUTION BEING TITRATED.

• Press Continue to begin the titration and Stop to abort it.

• At the end of the titration the instrument displays the concentration in ppm of SO2. The titration

curve can be viewed by pressing Plot ON. Press Plot OFF to exit this mode. For more informationabout this feature, see page 22.

Press Delete to delete the selected log from the memory.

Press Del.All to delete all records.

Press Info to see detailed information about the highlighted record.

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Press MENU then GLP.

The pump’s last calibration time, date and slope is displayed.

If a calibration hasn’t been performed, the message “Not Calibrated” will be displayed.

TITRATOR GLP INFORMATION

If Delete or Del.All is pressed the instrument will ask for confirmation.

Press Yes to delete the record or No to return to the previous screen.

Deleting a single record will renumber the list of records.

The selected record data and the titration curve data file name are displayed.

When a USB storage device is connected, the Export key is displayed. It saves the titration curvedata as a text file on the storage device using the displayed file name.

Use the ARROW keys when is displayed to scroll between the log records.

Press ESC to return to the previous screen.

Press Plot to visualize the titration curve or ESC to return to the previous screen. On the titrationcurve, the end point volume and mV are displayed. The titration data (Total Titrant Volume on thex-axis and mV on the y-axis) can be scanned through with the dotted line by using the ARROW keys.

To zoom on the titration curve press Zoom.

If the titrator log is empty, the message “No records available!” will be displayed.

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3332

Press Meter or Titrator to view the respective logs.

The instrument will display a list of all the records stored in the log.

Use the ARROW keys to scroll the list of records.

If the saved ORP measurements are out of range, the “<” or “>” symbols are displayed in frontof the reading.

Press Delete to delete the selected log from the memory.

Press Del.All to delete all records.

Press Info to see detailed information about the highlighted record.

Use ARROW keys when is displayed to scroll between the records.

If Delete or Del.All is pressed the instrument will ask for confirmation.

Press Yes to delete the record or No to return to the previous screen without deleting.

Deleting a single record will renumber the list of records.

If the ORP log is empty, the message “No records available!” will be displayed.

VIEW/DELETE RECORDED ORP DATA

To view or delete previously logged ORP records, press MENU then Recall to access meter logs.

When an external USB storage device is connected, the Export key is displayed. It saves themeter and titrator logs in two text format files on the storage device.

Press LOG to save the current reading.

During ORP measurements with stirrer on, the stirrer icon will be displayed. In case of a stirrermalfunction, the stirrer will stop and the stirrer icon will start blinking.

ORP MEASUREMENT

The HI 84500 can be used as an ORP meter for direct measurements.

Set the instrument to ORP meter. From titrator mode press Meter until mV units are displayed.

Rinse the ORP tip with distilled or deionized water.

Place ORP electrode into electrode holder.

For a faster response and to avoid cross-contamination of the samples, rinse the electrode tipwith a few drops of the solution to be tested before taking measurements.

Immerse the ORP sensor in the sample until the PTFE reference junction is completelysubmerged and stir gently for a few seconds.

When the reading becomes stable the (unstable measurement) symbol will disappear.

If the potential reading is less than -2000.0 mV or greater than 2000.0 mV the closest full-scalevalue will be displayed blinking.

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TROUBLESHOOTING GUIDE

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PC INTERFACE AND DATA TRANSFER

Data stored on the meter with the LOG function during mV measurement and titrations can betransferred from the meter to a USB stick using the Export function from the log recall menu.Two text files are transferred on the USB stick. These files can be used for further analysis on a PC.

The logged data can also be transferred from the instrument to the PC using a USB cable.Connect the USB cable and the following screen will be displayed.

Press Meter to generate the text file with Meter log data.

Press Titrator to generate the text file with Titrator log data.

Press Plot to generate the text files with Titration Plots.

The generated files are now visible and can be used fot further analysis.If the instrument has no logged Meter or Titrator records, the PC connected screen is displayed.

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If the bulb and/or junction is dry, soak the electrode in HI 70300L Storage Solution for at leastone hour.If the fill solution (electrolyte) is more than 2½ cm (1”) below the fill hole, add HI 7082 3.5MKCl Electrolyte Solution.For faster response, unscrew the fill hole screw during measurements.

STORAGE PROCEDURE

To minimize clogging and assure a quick response time, the glass bulb and junction of theelectrode should be kept moist and not allowed to dry out.

Replace the solution in the protective cap with a few drops of HI 70300L Storage Solution or,in its absence, HI 7082 Fill Solution. Follow the Preparation Procedure before takingmeasurements.

Note: NEVER STORE THE ELECTRODE IN DISTILLED OR DEIONIZED WATER.

PERIODIC MAINTENANCE

Inspect the electrode and the cable. The cable used for connection to the instrument must beintact and there must be no points of broken insulation on the cable or cracks on the electrodestem or bulb. Connectors must be perfectly clean and dry. If any scratches or cracks are present,replace the electrode. Rinse off any salt deposits with water.

PROBE MAINTENANCE

Refill the reference chamber with fresh electrolyte (HI 7082). Allow the electrode to standupright for 1 hour. Follow the Storage Procedure above.

CLEANING PROCEDURE

• Wine deposits Soak in Hanna HI 70635 cleaning solution for 15 minutes

• Wine stains Soak in Hanna HI 70636 cleaning solution for 15 minutes

IMPORTANT: After performing any of the cleaning procedures, rinse the electrode thoroughlywith distilled water, refill the reference chamber with fresh electrolyte and soak the electrode inHI 70300 Storage Solution for at least 1 hour before taking measurements.

ELECTRODE CONDITIONING AND MAINTENANCE

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PREPARATION PROCEDURE

Remove the protective cap of the ORP electrode (HI 3148B).

DO NOT BE ALARMED IF SALT DEPOSITS ARE PRESENT. This is normal with electrodes. They willdisappear when rinsed with distilled/deionized water.

During transport, tiny bubbles of air may have formed inside the glass bulb, affecting properfunctioning of the electrode. These bubbles can be removed by "shaking down" the electrode asyou would do with a glass thermometer.

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HI 84500 is guaranteed for two years against defects in workmanship and materials when usedfor it’s intended purpose and maintained according to instructions. Electrodes and probes areguaranteed for six months. This warranty is limited to repair or replacement free of charge.

Damage due to accidents, misuse, tampering or lack of prescribed maintenance is not covered.

If service is required, contact your dealer from whom you purchased the instrument. If underwarranty, report the model number, date of purchase, serial number and the nature of theproblem. If the repair is not covered by the warranty, you will be notified of the charges incurred.

If the instrument is to be returned to Hanna Instruments, first obtain a Returned GoodsAuthorization number from the Technical Service department and then send it with shipping costsprepaid. When shipping any instrument, make sure it is properly packed for complete protection.

To validate your warranty, fill out and return the enclosed warranty card within 14 days from thedate of purchase.

WARRANTY

Hanna Instruments reserves the right to modify the design, construction or appearance of its productswithout advance notice.

Before using this product, make sure that it is entirely suitable for your specific application and for theenvironment in which it is used.

Operation of this instrument may cause unacceptable interferences to other electronic equipment, thisrequiring the operator to take all necessary steps to correct interferences.

Any variation introduced by the user to the supplied equipment may degrade the instrument’s EMCperformance.

To avoid damages or burns, do not put the instrument in microwave ovens. For your’s and the instrument’s

safety do not use or store the instrument in hazardous environments.

RECOMMENDATION FOR USERS

REAGENTS

HI 84500-50 Low Range Titrant (230 mL)

HI 84500-51 High Range Titrant (230 mL)

HI 84500-55 Calibration Standard (120 mL)

HI 84500-60 Acid Reagent (230 mL)HI 84500-61 Alkaline Reagent (120 mL)

HI 84500-62 Stabilizer Packet (100 pcs.)

ELECTRODE TEST SOLUTION

HI 7021M ORP Test Solution (230 mL)

HI 7021L ORP Test Solution (500 mL)

ELECTRODE

HI 3148B ORP Electrode

ELECTRODE FILL SOLUTION

HI 7082 Electrode fill solution (4 x 30 mL)

ELECTRODE STORAGE SOLUTION

HI 70300L Electrode storage solution (500 mL)

CLEANING SOLUTION

HI 70635L Cleaning solution for wine deposits (500 mL)

HI 70636L Cleaning solution for wine stains (500 mL)

OTHER ACCESSORIES

HI 70500 Tube set with cap for titrant bottle, tip and valve

HI 71005/8 115 Vac to 12 Vdc, 800 mA

HI 71006/8 230 Vac to 12 Vdc, 800 mA

HI 731319 Stir bar (10 pcs., 25 x 7 mm)

HI 740036P Beaker 100 mL (10 pcs.)

HI 740037P Beaker 20 mL (10 pcs.)

HI 740236 5 mL Syringe for minititrator

HI 920013 PC Connection Cable

ACCESSORIES

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MAN84500 02/15Printed in ROMANIA

Hanna Instruments Inc.Highland Industrial Park584 Park East DriveWoonsocket, RI 02895 USA

Technical Support for CustomersTel. (800) 426 6287Fax (401) 765 7575E-mail [email protected]

Local Sales and Customer Service Office